#------------------------------------------------------------------------------
#$Date: 2016-03-24 17:09:42 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179679 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/01/7000110.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7000110
loop_
_publ_author_name
'Braun, Thomas'
'Steffen, Andreas'
'Schorlemer, Verena'
'Neumann, Beate'
'Stammler, Hans-Georg'
_publ_section_title
;
 Routes to unique palladium A-frame complexes with a bridging
 fluoro-ligand.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3331
_journal_page_last               3336
_journal_paper_doi               10.1039/b509032f
_journal_year                    2005
_chemical_formula_moiety         'C52 H50 F P4 Pd2, 2(C4 H8 O), F2 H'
_chemical_formula_sum            'C60 H67 F3 O2 P4 Pd2'
_chemical_formula_weight         1213.82
_chemical_name_systematic        ?
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.8150(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.6810(3)
_cell_length_b                   9.23800(10)
_cell_length_c                   25.2280(3)
_cell_measurement_reflns_used    8351
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      2.910
_cell_volume                     5444.70(11)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'KappaCCD '
_computing_data_reduction
'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL-PLUS (1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.042
_diffrn_reflns_av_sigmaI/netI    0.0315
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            57348
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    0.831
_exptl_absorpt_correction_T_max  0.9441
_exptl_absorpt_correction_T_min  0.8514
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2488
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.776
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         7922
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0259
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w=1/[σ²(Fo²)+(0.0277P)²+5.5484P] where
P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0607
_refine_ls_wR_factor_ref         0.0633
_reflns_number_gt                6861
_reflns_number_total             7922
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b509032f.txt
_cod_data_source_block           complex5cx2THF
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7000110
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.436491(5) 0.708743(12) 0.238097(4) 0.01098(4) Uani 1 1 d . . .
P1 P 0.417051(17) 0.76713(4) 0.144908(16) 0.01138(8) Uani 1 1 d . . .
P2 P 0.454751(17) 0.68453(4) 0.333107(16) 0.01125(8) Uani 1 1 d . . .
F1 F 0.5000 0.87688(14) 0.2500 0.0156(3) Uani 1 2 d S . .
F2 F 0.46512(4) 1.06254(11) 0.51119(4) 0.0225(2) Uani 1 1 d . . .
H2A H 0.5000 1.0000 0.5000 0.075(13) Uiso 1 2 d S . .
C1 C 0.37058(7) 0.66143(17) 0.08703(6) 0.0133(3) Uani 1 1 d . . .
C2 C 0.31189(7) 0.66391(18) 0.07880(7) 0.0159(3) Uani 1 1 d . . .
H2 H 0.2977 0.7186 0.1034 0.019 Uiso 1 1 calc R . .
C3 C 0.27404(7) 0.58722(19) 0.03501(7) 0.0185(3) Uani 1 1 d . . .
H3 H 0.2341 0.5903 0.0296 0.022 Uiso 1 1 calc R . .
C4 C 0.29441(7) 0.50587(19) -0.00097(7) 0.0198(3) Uani 1 1 d . . .
H4 H 0.2685 0.4537 -0.0310 0.024 Uiso 1 1 calc R . .
C5 C 0.35268(8) 0.5015(2) 0.00736(7) 0.0209(3) Uani 1 1 d . . .
H5 H 0.3667 0.4452 -0.0169 0.025 Uiso 1 1 calc R . .
C6 C 0.39092(7) 0.57883(19) 0.05100(7) 0.0184(3) Uani 1 1 d . . .
H6 H 0.4308 0.5754 0.0563 0.022 Uiso 1 1 calc R . .
C7 C 0.38424(6) 0.94618(17) 0.13281(6) 0.0136(3) Uani 1 1 d . . .
C8 C 0.37165(7) 1.01194(18) 0.08022(7) 0.0163(3) Uani 1 1 d . . .
H8 H 0.3781 0.9613 0.0500 0.020 Uiso 1 1 calc R . .
C9 C 0.34962(7) 1.15180(19) 0.07241(7) 0.0187(3) Uani 1 1 d . . .
H9 H 0.3411 1.1967 0.0368 0.022 Uiso 1 1 calc R . .
C10 C 0.34005(7) 1.22621(18) 0.11650(7) 0.0194(3) Uani 1 1 d . . .
H10 H 0.3253 1.3220 0.1110 0.023 Uiso 1 1 calc R . .
C11 C 0.35202(7) 1.16107(19) 0.16841(7) 0.0192(3) Uani 1 1 d . . .
H11 H 0.3453 1.2119 0.1984 0.023 Uiso 1 1 calc R . .
C12 C 0.37391(7) 1.02079(18) 0.17658(7) 0.0166(3) Uani 1 1 d . . .
H12 H 0.3818 0.9759 0.2122 0.020 Uiso 1 1 calc R . .
C13 C 0.39829(7) 0.74975(18) 0.35919(6) 0.0135(3) Uani 1 1 d . . .
C14 C 0.41002(7) 0.82492(19) 0.40954(7) 0.0184(3) Uani 1 1 d . . .
H14 H 0.4484 0.8490 0.4304 0.022 Uiso 1 1 calc R . .
C15 C 0.36563(7) 0.8648(2) 0.42932(7) 0.0210(3) Uani 1 1 d . . .
H15 H 0.3738 0.9171 0.4634 0.025 Uiso 1 1 calc R . .
C16 C 0.30971(7) 0.8287(2) 0.39954(8) 0.0226(4) Uani 1 1 d . . .
H16 H 0.2797 0.8532 0.4138 0.027 Uiso 1 1 calc R . .
C17 C 0.29751(7) 0.7566(2) 0.34880(8) 0.0244(4) Uani 1 1 d . . .
H17 H 0.2590 0.7336 0.3280 0.029 Uiso 1 1 calc R . .
C18 C 0.34146(7) 0.71804(19) 0.32829(7) 0.0195(3) Uani 1 1 d . . .
H18 H 0.3329 0.6700 0.2932 0.023 Uiso 1 1 calc R . .
C19 C 0.47053(6) 0.50333(17) 0.36218(6) 0.0134(3) Uani 1 1 d . . .
C20 C 0.46156(7) 0.46359(19) 0.41225(7) 0.0173(3) Uani 1 1 d . . .
H20 H 0.4453 0.5309 0.4313 0.021 Uiso 1 1 calc R . .
C21 C 0.47648(7) 0.32544(19) 0.43420(7) 0.0207(3) Uani 1 1 d . . .
H21 H 0.4704 0.2987 0.4682 0.025 Uiso 1 1 calc R . .
C22 C 0.50026(8) 0.22681(19) 0.40658(8) 0.0220(4) Uani 1 1 d . . .
H22 H 0.5107 0.1329 0.4218 0.026 Uiso 1 1 calc R . .
C23 C 0.50884(8) 0.26525(19) 0.35649(8) 0.0213(3) Uani 1 1 d . . .
H23 H 0.5250 0.1976 0.3375 0.026 Uiso 1 1 calc R . .
C24 C 0.49376(7) 0.40266(18) 0.33438(7) 0.0164(3) Uani 1 1 d . . .
H24 H 0.4993 0.4283 0.3000 0.020 Uiso 1 1 calc R . .
C25 C 0.48383(6) 0.79882(17) 0.12920(6) 0.0134(3) Uani 1 1 d . . .
H25A H 0.4950 0.9013 0.1376 0.016 Uiso 1 1 calc R . .
H25B H 0.4760 0.7845 0.0885 0.016 Uiso 1 1 calc R . .
C26 C 0.37900(7) 0.54242(18) 0.22016(7) 0.0176(3) Uani 1 1 d . . .
H26A H 0.3402 0.5812 0.2038 0.026 Uiso 1 1 calc R . .
H26B H 0.3817 0.4898 0.2546 0.026 Uiso 1 1 calc R . .
H26C H 0.3875 0.4764 0.1935 0.026 Uiso 1 1 calc R . .
O1 O 0.29313(8) 0.2286(2) 0.27571(6) 0.0460(4) Uani 1 1 d . . .
C27 C 0.26724(9) 0.3458(2) 0.29602(9) 0.0335(4) Uani 1 1 d . . .
H27A H 0.2265 0.3242 0.2907 0.040 Uiso 1 1 calc R . .
H27B H 0.2693 0.4362 0.2757 0.040 Uiso 1 1 calc R . .
C28 C 0.30060(10) 0.3618(2) 0.35790(8) 0.0346(5) Uani 1 1 d . . .
H28A H 0.2754 0.3930 0.3794 0.042 Uiso 1 1 calc R . .
H28B H 0.3324 0.4318 0.3640 0.042 Uiso 1 1 calc R . .
C29 C 0.32294(9) 0.2090(2) 0.37383(9) 0.0313(4) Uani 1 1 d . . .
H29A H 0.3577 0.2089 0.4072 0.038 Uiso 1 1 calc R . .
H29B H 0.2935 0.1462 0.3810 0.038 Uiso 1 1 calc R . .
C30 C 0.33621(9) 0.1621(3) 0.32168(9) 0.0357(5) Uani 1 1 d . . .
H30A H 0.3748 0.1953 0.3232 0.043 Uiso 1 1 calc R . .
H30B H 0.3345 0.0554 0.3179 0.043 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C26 Pd1 F1 174.11(5) . . ?
C26 Pd1 P2 92.66(5) . . ?
F1 Pd1 P2 92.038(11) . . ?
C26 Pd1 P1 92.80(5) . . ?
F1 Pd1 P1 82.906(12) . . ?
P2 Pd1 P1 171.997(15) . . ?
C26 Pd1 Pd1 130.71(5) . 2_655 ?
F1 Pd1 Pd1 46.04(2) . 2_655 ?
P2 Pd1 Pd1 87.162(11) . 2_655 ?
P1 Pd1 Pd1 93.702(11) . 2_655 ?
C1 P1 C7 102.77(7) . . ?
C1 P1 C25 106.79(7) . . ?
C7 P1 C25 101.54(7) . . ?
C1 P1 Pd1 124.17(5) . . ?
C7 P1 Pd1 108.53(5) . . ?
C25 P1 Pd1 110.53(5) . . ?
C19 P2 C13 104.33(7) . . ?
C19 P2 C25 106.62(7) . 2_655 ?
C13 P2 C25 102.82(7) . 2_655 ?
C19 P2 Pd1 116.99(5) . . ?
C13 P2 Pd1 115.31(5) . . ?
C25 P2 Pd1 109.53(5) 2_655 . ?
Pd1 F1 Pd1 87.92(5) 2_655 . ?
C2 C1 C6 119.03(14) . . ?
C2 C1 P1 117.72(12) . . ?
C6 C1 P1 123.25(12) . . ?
C3 C2 C1 120.63(15) . . ?
C2 C3 C4 120.17(15) . . ?
C5 C4 C3 119.52(15) . . ?
C4 C5 C6 120.67(16) . . ?
C5 C6 C1 119.98(15) . . ?
C12 C7 C8 119.67(15) . . ?
C12 C7 P1 120.07(12) . . ?
C8 C7 P1 120.20(12) . . ?
C9 C8 C7 119.64(15) . . ?
C10 C9 C8 120.34(15) . . ?
C11 C10 C9 120.16(15) . . ?
C10 C11 C12 119.90(15) . . ?
C7 C12 C11 120.28(15) . . ?
C14 C13 C18 119.26(15) . . ?
C14 C13 P2 122.33(12) . . ?
C18 C13 P2 118.37(12) . . ?
C15 C14 C13 120.16(15) . . ?
C16 C15 C14 120.28(16) . . ?
C15 C16 C17 119.92(16) . . ?
C16 C17 C18 120.22(16) . . ?
C17 C18 C13 120.09(16) . . ?
C24 C19 C20 119.30(15) . . ?
C24 C19 P2 118.69(11) . . ?
C20 C19 P2 121.98(12) . . ?
C21 C20 C19 120.04(16) . . ?
C22 C21 C20 120.17(16) . . ?
C21 C22 C23 120.07(16) . . ?
C24 C23 C22 119.88(16) . . ?
C23 C24 C19 120.53(15) . . ?
P1 C25 P2 116.32(8) . 2_655 ?
C27 O1 C30 109.52(16) . . ?
O1 C27 C28 106.52(17) . . ?
C27 C28 C29 102.22(17) . . ?
C30 C29 C28 101.34(17) . . ?
O1 C30 C29 105.53(17) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C26 2.0407(16) . ?
Pd1 F1 2.1578(10) . ?
Pd1 P2 2.3025(4) . ?
Pd1 P1 2.3066(4) . ?
Pd1 Pd1 2.9956(2) 2_655 ?
P1 C1 1.8223(16) . ?
P1 C7 1.8236(16) . ?
P1 C25 1.8387(15) . ?
P2 C19 1.8187(16) . ?
P2 C13 1.8247(16) . ?
P2 C25 1.8405(16) 2_655 ?
F1 Pd1 2.1578(10) 2_655 ?
F2 H2A 1.1452(10) . ?
C1 C2 1.396(2) . ?
C1 C6 1.398(2) . ?
C2 C3 1.389(2) . ?
C3 C4 1.391(2) . ?
C4 C5 1.385(2) . ?
C5 C6 1.394(2) . ?
C7 C12 1.393(2) . ?
C7 C8 1.400(2) . ?
C8 C9 1.391(2) . ?
C9 C10 1.391(2) . ?
C10 C11 1.384(2) . ?
C11 C12 1.394(2) . ?
C13 C14 1.394(2) . ?
C13 C18 1.398(2) . ?
C14 C15 1.392(2) . ?
C15 C16 1.383(2) . ?
C16 C17 1.387(2) . ?
C17 C18 1.391(2) . ?
C19 C24 1.395(2) . ?
C19 C20 1.400(2) . ?
C20 C21 1.393(2) . ?
C21 C22 1.387(3) . ?
C22 C23 1.393(2) . ?
C23 C24 1.388(2) . ?
C25 P2 1.8404(16) 2_655 ?
O1 C27 1.433(3) . ?
O1 C30 1.434(3) . ?
C27 C28 1.519(3) . ?
C28 C29 1.521(3) . ?
C29 C30 1.518(3) . ?
